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In this study, α-Bi2O3/g-C3N4 nanocomposite with direct Z-scheme was successfully prepared through calcination of BiOCOOH/g-C3N4 precursor at different temperature. Meanwhile, the effect of calcination temperature on the physicochemical properties of α- Bi2O3/g-C3N4was studied. All results confirmed that calcination temperature greatly influences structural, morphology, surface states, photoelectrochemical property and photocatalytic (PC) performance of α- Bi2O3/g-C3N4 composite. Furthermore, the α- Bi2O3/g-C3N4 composite was applied as photocatalyst to degrade amido black 10B dye under visible light irradiation. It was found that the composite synthesized at 400 °C exhibited the highest PC performance due to the intense visible light absorbance and high separation efficiency of electron and hole pairs.Besides, the possible PC mechanism was proposed that the photo-generated charge carrier migration in α- Bi2O3/g-C3N4 photocatalyst followed a Z-scheme structure. Finally, the stability test also manifest that the α- Bi2O3/g-C3N4 composite photocatalyst has good stability and reusability, which was a promising candidate for wastewater treatment.